(57) A continuous process for recovering highly pure acetonitrile from crude acetonitrile containing acetonitrile, water, HCN and heavy organics, said process comprising:

(1) distilling said crude acetonitrile in a first distillation zone at a first pressure at or above 1 atmosphere to remove HCN therefrom and produce a first acetonitrile/water azeotrope and a first bottoms product containing water,

(2) distilling said first azeotrope in a second distillation zone at a second pressure less than 1 atmosphere to separate said first azeotrope into a second bottoms product containing water and a second acetonitrile/water azeotrope having a greater acetonitrile concentration than said first azeotrope, and

(3) distilling said second acetonitrile/water azeotrope in a third distillation zone at a third pressure above 1 atmosphere to produce a third acetonitrile/water azeotrope containing substantially all of the water in said second azeotrope, third bottoms product comprising acetonitrile and heavy organics and a sidestream comprising said highly pure acetonitrile.

This process enables one to obtain acetonitrile in 99+% purity. It is based upon a continuous distillation process carried out in three stages at three different pressures.